场地有机物污染土壤的脉冲放电等离子体修复方法和机理研究
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摘要
随着现代工业生产的快速发展和城市化进程的加快,大批化工企业搬迁或退役导致企业周边场地存在严重污染,特别是有机物污染。这些污染场地面临快速的商业化开发利用,场地土壤中残留的大量有机污染物严重危害人居环境安全健康,因此,亟需对这类污染土壤进行高效快速的修复。然而,传统土壤修复方法无法满足高效快速的修复要求,迫切需要发展高效快速的有机物污染土壤修复方法。放电等离子体技术作为一种高级氧化技术,在环境污染物降解方面具有效率高、速度快、对污染物无选择性、以及无二次污染等优点,受到研究者的广泛关注。基于此,本论文提出采用脉冲放电等离子体技术修复有机物污染土壤,主要围绕脉冲放电等离子体修复有机污染土壤过程中污染物的降解特性、活性物质的产生和作用途径、污染物的降解机理、污染物和活性物质的扩散迁移行为、放电等离子体与催化剂的协同作用等方面开展研究。主要的工作及研究结果如下：
1.采用脉冲放电等离子体修复五氯酚(pentachlorophenol, PCP)污染土壤,借助电气参数、反应器结构参数、载气参数和土壤特征考察了土壤中PCP降解特性。发现：脉冲放电等离子体对土壤中PCP具有快速高效的降解能力,放电处理60min, PCP降解率高达83.5%。增加脉冲峰值电压、脉冲重复频率和减小电极间距促进PCP降解；不同载气中PCP降解梯度为：氧气>空气>氮气；存在最优的气体流量使得上壤中PCP降解效果较好：土壤有机质抑制PCP降解；碱性土壤和适当土壤湿度有利于PCP降解。
2.通过活性物质的定性和定量分析,并借助总有机碳分析仪(TOC)、紫外-可见光谱、傅立叶变换红外光谱(FT-IR)、离子色谱(IC)以及高效液相色谱-质谱联用(HPLC/MS)等分析了PCP降解产物,探讨了PCP污染土壤修复机理。发现含氧活性基团(如03,·OH自由基等)氧化是修复PCP污染土壤主要的作用途径。强氧化性活性物质攻击PCP的C-Cl键,产生羟基化中间产物,伴随脱氯反应的发生,这些中间产物被进一步氧化开环,生成小分子有机酸,并最终矿化为C02和H20。
3.研究了脉冲放电等离子体对七层中对硝基苯酚(p-nitrophenol, PNP)的降解特性和活性物质的扩散行为,考察了媒质材料、土壤特性、脉冲峰值电压和PNP初始浓度等参数对PNP降解和主要活性物质O3扩散穿透能力的影响。结果表明：不同土层中氧化环境差异,使得土层中PNP降解、矿化和中间产物显著不同。PNP降解率随土层增加而降低。上层中PNP降解受土壤特征、脉冲峰值电压和污染物浓度影响。土壤内含物、土壤特性和O3浓度影响O3在土壤中的扩散。
4.采川脉冲放电等离子体修复PCP和PNP复合污染土壤，探讨了污染组分之间的相互影响行为。发现：脉冲放电等离子体能够高效修复复合污染土壤，一定条件下土壤中PCP和PNP降解率分别高达94.1%和86.0%。复合污染土壤修复过程中，PCP和PNP相互制约。提高脉冲峰值电压和土壤pH可以显著提高复合污染土壤修复效果。
5.采用脉冲放电等离子体TiO2催化联合体系修复PNP污染土壤，借助脉冲峰值电压、土壤pH和载气湿度研究了联合体系中PNP的降解特性。通过比较单一放电体系和联合体系中PNP降解、矿化、活性物质生成、中间产物演化等差异，探讨了联合体系对PNP污染土壤的协同修复机理。研究发现：与单一放电体系相比，联合体系产生了更多的活性物质，促进了PNP降解和矿化，并加速中间产物的生成与矿化。
With the quick development of industrial production and urbanization, lots of relocated or closed industrial enterprises caused serious soil pollution, especially organic pollutants contaminated soil. These polluted sites need quick commercial utilization, but lots of organic pollutants in soil bring dangers to people's living. Therefore, rapid and high efficient remediation for these sites is becoming a necessary. Lots of methods had been proposed, such as physical remediation, traditional chemical remediation, and bioremediation; however, there exist some drawbacks, and can not meet remediation requirements of high efficiency and speed, and thus development of new methods for soil remediation is important. Discharge plasma, one of advanced oxidation processes, has been received great attention in pollution control, showing advantages of high efficiency, high speed, no selective for pollutants, and no secondary pollution. Therefore, pulsed discharge plasma was proposed to remediate organic pollutants contaminated soil in this paper. The main work was conducted in terms of pollutants degradation characteristics, generation and roles of active species, pollutants degradation mechanisms, transport of pollutants and active species in soil, synthetic effects of discharge plasma and catalyst for pollutants removal. The detailed work and the summarized results are as follows:
1. Pulsed discharge plasma was used to remediate pentachlorophenol (PCP) contaminated soil. PCP degradation characteristics in soil were studied by evaluating the effects of electrical parameters, reactor configuration parameters, carrier gas atmospheres, and soil properties on its degradation. The experimental results showed that pulsed discharge plasma was an efficient and quick method for PCP contaminated soil remediation.83.5%of PCP could be removed within60min's discharge treatment. Increasing pulsed discharge voltage and pulsed frequency, and decreasing electrode distance could improve PCP removal. The greatest PCP removal efficiency was obtained in O2atmosphere, followed by air atmosphere, and the lowest in N2atmosphere. There existed an optimal value for gas flow rate to obtain high PCP removal. Soil organic matter inhibited PCP removal. Alkaline soil and certain water content in soil benefited PCP removal.
2. By qualitative and quantitative analysis of active species, and analysis of PCP degradation intermediates by TOC, UV-VIS, FT-IR, IC, and HPLC-MS, PCP degradation mechanisms were proposed. O-containing active species oxidation (such as O3and·OH) was the main process for PCP degradation. The attacks of these active species to C-Cl bonds in PCP molecule initiated PCP degradation process, generating hydroxylated intermediates, accompanied by dechlorination reactions, and then the hydroxylated intermediates were further degraded into small organic acids, CO2and H2O.
3.p-Nitrophenol (PNP) degradation in soil by pulsed discharge plasma was investigated, and the transfer of O3in soil was also studied. The effects of matrix, soil properties, discharge voltage, and PNP concentration on PNP degradation and O3breakthrough were evaluated. The results presented that due to the different oxidative conditions in soil layers, PNP degradation, mineralization, and intermediates were quite different in different soil layers. PNP degradation efficiency decreased with increase of soil depth. Soil properties, discharge voltage, and PNP concentration affect PNP degradation. Soil organic matter and metal oxides, soil properties, and O3concentration affect its diffusion in soil layer.
4.Pulsed discharge plasma was used to remediate PCP and PNP mixtures contaminated soil. The mutual effects between reactants were discussed. The results showed that pulsed discharge plasma presented great performance for mixtures contaminated soil remediation.86.0%of PNP and94.1%of PCP could be removed in certain conditions. There existed mutual suppressant effects between PCP and PNP during soil remediation. Alkaline soil and high discharge voltage were both beneficial for mixtures contaminated soil remediation.
5. Pulsed discharge plasma and TiO2catalyst were combined to remediate PNP contaminated soil. The effects of discharge voltage, soil pH and gas moisture on PNP degradation were studied. The synthetic mechanisms were discussed by comparing PNP degradation, mineralization, active species generation, and evolution of intermediates with single discharge system. The results showed that more active species were generated in pulsed discharge plasma/TiO2system, resulting in higher PNP degradation and mineralization, and then accelerated generation and mineralization of intermediates.
1.采用脉冲放电等离子体修复五氯酚(pentachlorophenol, PCP)污染土壤,借助电气参数、反应器结构参数、载气参数和土壤特征考察了土壤中PCP降解特性。发现：脉冲放电等离子体对土壤中PCP具有快速高效的降解能力,放电处理60min, PCP降解率高达83.5%。增加脉冲峰值电压、脉冲重复频率和减小电极间距促进PCP降解；不同载气中PCP降解梯度为：氧气>空气>氮气；存在最优的气体流量使得上壤中PCP降解效果较好：土壤有机质抑制PCP降解；碱性土壤和适当土壤湿度有利于PCP降解。
2.通过活性物质的定性和定量分析,并借助总有机碳分析仪(TOC)、紫外-可见光谱、傅立叶变换红外光谱(FT-IR)、离子色谱(IC)以及高效液相色谱-质谱联用(HPLC/MS)等分析了PCP降解产物,探讨了PCP污染土壤修复机理。发现含氧活性基团(如03,·OH自由基等)氧化是修复PCP污染土壤主要的作用途径。强氧化性活性物质攻击PCP的C-Cl键,产生羟基化中间产物,伴随脱氯反应的发生,这些中间产物被进一步氧化开环,生成小分子有机酸,并最终矿化为C02和H20。
3.研究了脉冲放电等离子体对七层中对硝基苯酚(p-nitrophenol, PNP)的降解特性和活性物质的扩散行为,考察了媒质材料、土壤特性、脉冲峰值电压和PNP初始浓度等参数对PNP降解和主要活性物质O3扩散穿透能力的影响。结果表明：不同土层中氧化环境差异,使得土层中PNP降解、矿化和中间产物显著不同。PNP降解率随土层增加而降低。上层中PNP降解受土壤特征、脉冲峰值电压和污染物浓度影响。土壤内含物、土壤特性和O3浓度影响O3在土壤中的扩散。
4.采川脉冲放电等离子体修复PCP和PNP复合污染土壤，探讨了污染组分之间的相互影响行为。发现：脉冲放电等离子体能够高效修复复合污染土壤，一定条件下土壤中PCP和PNP降解率分别高达94.1%和86.0%。复合污染土壤修复过程中，PCP和PNP相互制约。提高脉冲峰值电压和土壤pH可以显著提高复合污染土壤修复效果。
5.采用脉冲放电等离子体TiO2催化联合体系修复PNP污染土壤，借助脉冲峰值电压、土壤pH和载气湿度研究了联合体系中PNP的降解特性。通过比较单一放电体系和联合体系中PNP降解、矿化、活性物质生成、中间产物演化等差异，探讨了联合体系对PNP污染土壤的协同修复机理。研究发现：与单一放电体系相比，联合体系产生了更多的活性物质，促进了PNP降解和矿化，并加速中间产物的生成与矿化。
With the quick development of industrial production and urbanization, lots of relocated or closed industrial enterprises caused serious soil pollution, especially organic pollutants contaminated soil. These polluted sites need quick commercial utilization, but lots of organic pollutants in soil bring dangers to people's living. Therefore, rapid and high efficient remediation for these sites is becoming a necessary. Lots of methods had been proposed, such as physical remediation, traditional chemical remediation, and bioremediation; however, there exist some drawbacks, and can not meet remediation requirements of high efficiency and speed, and thus development of new methods for soil remediation is important. Discharge plasma, one of advanced oxidation processes, has been received great attention in pollution control, showing advantages of high efficiency, high speed, no selective for pollutants, and no secondary pollution. Therefore, pulsed discharge plasma was proposed to remediate organic pollutants contaminated soil in this paper. The main work was conducted in terms of pollutants degradation characteristics, generation and roles of active species, pollutants degradation mechanisms, transport of pollutants and active species in soil, synthetic effects of discharge plasma and catalyst for pollutants removal. The detailed work and the summarized results are as follows:
1. Pulsed discharge plasma was used to remediate pentachlorophenol (PCP) contaminated soil. PCP degradation characteristics in soil were studied by evaluating the effects of electrical parameters, reactor configuration parameters, carrier gas atmospheres, and soil properties on its degradation. The experimental results showed that pulsed discharge plasma was an efficient and quick method for PCP contaminated soil remediation.83.5%of PCP could be removed within60min's discharge treatment. Increasing pulsed discharge voltage and pulsed frequency, and decreasing electrode distance could improve PCP removal. The greatest PCP removal efficiency was obtained in O2atmosphere, followed by air atmosphere, and the lowest in N2atmosphere. There existed an optimal value for gas flow rate to obtain high PCP removal. Soil organic matter inhibited PCP removal. Alkaline soil and certain water content in soil benefited PCP removal.
2. By qualitative and quantitative analysis of active species, and analysis of PCP degradation intermediates by TOC, UV-VIS, FT-IR, IC, and HPLC-MS, PCP degradation mechanisms were proposed. O-containing active species oxidation (such as O3and·OH) was the main process for PCP degradation. The attacks of these active species to C-Cl bonds in PCP molecule initiated PCP degradation process, generating hydroxylated intermediates, accompanied by dechlorination reactions, and then the hydroxylated intermediates were further degraded into small organic acids, CO2and H2O.
3.p-Nitrophenol (PNP) degradation in soil by pulsed discharge plasma was investigated, and the transfer of O3in soil was also studied. The effects of matrix, soil properties, discharge voltage, and PNP concentration on PNP degradation and O3breakthrough were evaluated. The results presented that due to the different oxidative conditions in soil layers, PNP degradation, mineralization, and intermediates were quite different in different soil layers. PNP degradation efficiency decreased with increase of soil depth. Soil properties, discharge voltage, and PNP concentration affect PNP degradation. Soil organic matter and metal oxides, soil properties, and O3concentration affect its diffusion in soil layer.
4.Pulsed discharge plasma was used to remediate PCP and PNP mixtures contaminated soil. The mutual effects between reactants were discussed. The results showed that pulsed discharge plasma presented great performance for mixtures contaminated soil remediation.86.0%of PNP and94.1%of PCP could be removed in certain conditions. There existed mutual suppressant effects between PCP and PNP during soil remediation. Alkaline soil and high discharge voltage were both beneficial for mixtures contaminated soil remediation.
5. Pulsed discharge plasma and TiO2catalyst were combined to remediate PNP contaminated soil. The effects of discharge voltage, soil pH and gas moisture on PNP degradation were studied. The synthetic mechanisms were discussed by comparing PNP degradation, mineralization, active species generation, and evolution of intermediates with single discharge system. The results showed that more active species were generated in pulsed discharge plasma/TiO2system, resulting in higher PNP degradation and mineralization, and then accelerated generation and mineralization of intermediates.
引文
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